Positron annihilation technique is a well known technique to characterize the defects in a material. These defects can be identified by positron annihilation lifetime and coincidence Doppler broadening of positron annihilation radiation measurement. In this chapter we report the room temperature positron annihilation lifetime for single crystalline ZnO. From our study it is confirmed that the present crystal contains VZn–hydrogen complexes with low open volumes. Another important nuclear solid technique is the Mossbauer Spectroscopic technique which has been used to probe the local magnetic properties of a solid. Here we have summarized Mossbauer spectroscopic studies on ferrites.